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Hydrazine → HCID 86608309, 화합물

HRID 2234043
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HRID 2234043 반응식
C(N(C(C)C)CC)(C)C.CN(C(O[N:18]1[N:26]=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C1C=NC2N(O)N=NC=2C=1.[Cl:44][C:45]1[CH:46]=[C:47]([CH:51]=[C:52]([N:54]2[CH2:59][CH2:58][CH:57]([NH:60][C:61]([C:63]3[NH:64][C:65]([CH3:70])=[C:66]([Cl:69])[C:67]=3[Cl:68])=[O:62])[CH2:56][CH2:55]2)[N:53]=1)[C:48]([OH:50])=O.NN>CN(C=O)C>[Cl:68][C:67]1[C:66]([Cl:69])=[C:65]([CH3:70])[NH:64][C:63]=1[C:61]([NH:60][CH:57]1[CH2:56][CH2:55][N:54]([C:52]2[CH:51]=[C:47]([C:48]([NH:18][NH2:26])=[O:50])[CH:46]=[C:45]([Cl:44])[N:53]=2)[CH2:59][CH2:58]1)=[O:62]
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7

반응물 5

HCID 9321HydrazineHCID 81531DiisopropylethylamineHCID 181649HOAtHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 57397809HCID 57397809, 화합물

생성물 1

HCID 86608309HCID 86608309, 화합물
수율 56.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Diisopropylethylamine (0.043 ml, 0.25 mmol), HATU (0.048 g, 0.12 mmol) and HOAT (0.017 g 0.12 mmol) were added to a stirred solution of 2-chloro-6-(4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)isonicotinic acid (Example 153; 0.055 g, 0.12 mmol) in DMF (2 ml). The resultant solution was stirred for 5 mins and hydrazine (0.04 ml, 0.12 mmol) was added. The mixture was stirred at room temperature for 14 h, partitioned between water and EtOAc. The layers were separated and the organic layer was washed with water two more times. The organic phase was dried over magnesium sulfate and concentrated to give the title compound (30 mg).

후처리

  1. custompartitioned between water and EtOAc
  2. customThe layers were separated
  3. washthe organic layer was washed with water two more times
  4. dry with materialThe organic phase was dried over magnesium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d429d1d995ff49c7a8c365685292bed6
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07709503B2

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